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If your ex forced you to keep his stuff for two years, a judge isn't going to be too sympathetic if he now claims he can't find his prized high school debate trophy. But your idea that he sign a receipt is a good one, and it should include an itemized list of all the property.
There is always the chance he will refuse to sign the receipt. If he does, you'll have to hand over the property anyway. But having a friend or neighbor present when your ex-husband comes for his things is a good idea, so that there's a witness to what you gave him, and also to prevent him from doing anything irrational. If he is a real hothead, you can ask your local police department for what they call a "civil standby." If they have an officer available, most police departments are happy to dispatch the officer to keep an eye on you for a short while. Obviously, scheduling an exchange for a Friday night is not a good idea because the police are likely to be busy dealing with more pressing problems.
Regardless of how you choose to handle the transfer, take some pictures -- or a video -- of the items you're going to give to your ex. Then, if doesn't cause too much of a problem, take some more of him loading them into his car. These pictures will come in very handy if he ever does call you into court.